Abstract: The solid complex of uranyl nitrate with dibenzo-24-crown-8 (DB24C8) , having a 2:1 stoichiometry UO2(NO3)22·DB24C8·4H2O, has been synthe-sized in anhydrous acetonitrile solution and characterized by elemental analysis, IR and UV spectra, thermogravimetric(TG) and differential thermal analyses, X-ray powder diffraction, and so on.